CN112592296B - Method for producing sodium isethionate by continuous reaction - Google Patents
Method for producing sodium isethionate by continuous reaction Download PDFInfo
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Abstract
The invention discloses a method for producing sodium isethionate by continuous reaction, which comprises the steps of carrying out addition reaction on sodium bisulfite aqueous solution and ethylene oxide serving as raw materials, firstly, mixing the sodium bisulfite aqueous solution with a certain concentration and the ethylene oxide with a certain flow rate at a certain flow rate, and allowing the mixture to stay for a period of time from a first reactor; mixing the first-stage reaction liquid with ethylene oxide at a certain flow rate, then feeding the mixture into a second reactor, staying for a period of time, then feeding the mixture into a third reactor and a fourth reactor respectively, adding an acidic substance into the fourth reactor to adjust the pH value to 7.0-8.0, and finally discharging. The method divides the addition reaction into at least four stages, accurately regulates and controls the process parameters of each stage, effectively reduces the hydrolysis rate of the ethylene oxide and the content of byproducts such as ethylene glycol, polyethylene glycol and the like in the product, not only improves the yield of the sodium isethionate, but also avoids subsequent purification process, and is more convenient for other uses.
Description
Technical Field
The invention relates to the field of preparation of sodium isethionate, in particular to a method for producing sodium isethionate by continuous reaction.
Background
The hydroxyethyl sodium sulfonate is a main raw material for producing the coconut oil base hydroxyethyl sodium sulfonate, and meanwhile, the product is widely used in the industries of electroplating, detergents and the like. Can be used as detergent for wool spinning products, intermediate for daily chemical products (such as shampoo and high-grade soap), pharmaceutical raw material and intermediate for fine chemical products.
At present, sodium isethionate is mainly prepared by addition reaction of sodium bisulfite and Ethylene Oxide (EO), and the widely adopted production process is as follows:
preparing 30-40 wt% water solution from sodium bisulfite, nitrogen replacing, heating, adding epoxy ethane at 60-90 deg.C, controlling the temperature at 80-100 deg.C and the pressure at 0-0.3 Mpa. After adding a certain amount of ethylene oxide, curing for 30-120 minutes at 90-100 ℃ to obtain a coarse product of sodium isethionate with mass concentration of 40-45%, wherein the impurity content is 1.5-2.0%, the coarse product mainly comprises ethylene glycol and derivatives thereof, and the hydrolysis rate of the ethylene oxide is about 1.0-2.0%. The presence of these impurities can affect the quality and yield of the product for further synthesis of sodium isethionate derivatives, and therefore, it is desirable to reduce the level of impurities in the product sodium isethionate.
Chinese patent publication No. CN 111320558A discloses a method for synthesizing taurine, which comprises performing an addition reaction between an aqueous solution of sodium bisulfite and liquid ethylene oxide to obtain an addition reaction solution containing sodium isethionate; the temperature and pressure of the addition reaction are as follows: 20-100 ℃, 0.5-5 bar and 10-120 min of reaction time. The addition reaction liquid contains byproducts (mainly ethylene glycol and polyethylene glycol), so the addition reaction liquid is further filtered by a nanofiltration membrane, and finally the sodium isethionate is separated from the byproducts by continuous circulating filtration.
Chinese patent document with application publication No. CN 102050764A discloses a method for purifying sodium isethionate, specifically discloses a method for purifying sodium isethionate by taking newly-prepared 30-40 wt% sodium bisulfite aqueous solution and ethylene oxide as raw materials, feeding the prepared 40-45 wt% crude product into a first-effect evaporator, concentrating to 55-60 wt% at 80-120 ℃, feeding into a second-effect evaporator, further concentrating and evaporating to 72-75 wt% at 100-130 ℃, then feeding the concentrated solution into a continuous crystallizer, recrystallizing for 1-6 h at 20-80 ℃, centrifugally separating crystal slurry, feeding the solid into the next process, respectively recovering mother liquor and crystallizing residual liquor; the purification is finished when the ethylene glycol content in the product reaches 0.1% by weight or less.
In the processes, the impurity content in the product sodium isethionate is reduced by a post-treatment mode, the production procedures are prolonged, the generation of three wastes is increased, and the production cost is greatly increased.
Disclosure of Invention
Aiming at the problems, the invention discloses a method for producing sodium isethionate by continuous reaction, which effectively reduces the hydrolysis rate of ethylene oxide and the content of byproducts such as ethylene glycol, polyethylene glycol and the like in products by accurately regulating and controlling the process flow and process parameters, improves the yield of the sodium isethionate, avoids subsequent purification process and is more convenient for other uses.
The specific technical scheme is as follows:
a method for producing sodium isethionate by continuous reaction takes sodium bisulfite aqueous solution and ethylene oxide as raw materials to carry out addition reaction, the addition reaction is divided into at least four stages to carry out, and the method specifically comprises the following steps:
the first stage is as follows: and (2) introducing an aqueous sodium bisulfite solution and ethylene oxide into a first reactor, and controlling the feeding molar ratio of the sodium bisulfite to the ethylene oxide to be 1:0.7 to 0.85, controlling the pH value in the reactor to be 5.5 to 6.0 and the temperature to be 25 to 35 ℃, and discharging after staying for a period of time;
and a second stage: and (3) introducing the material prepared in the first stage into a second reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the second stage to be 1:0.05 to 0.2, controlling the pH value in the reactor to be 6.0 to 6.5 and the temperature to be 35 to 45 ℃, and discharging after staying for a period of time;
and a third stage: and (3) introducing the material prepared in the second stage into a third reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the third stage to be 1:0.05 to 0.1, controlling the pH value in the reactor to be 6.5 to 7.0 and the temperature to be 45 to 55 ℃, and discharging after staying for a period of time;
a fourth stage: and (3) introducing the material prepared in the third stage into a fourth reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the fourth stage to be 1:0.05 to 0.1, and adjusting the pH value in the reactor to 7.0 to 8.0 and the temperature to 55 to 70 ℃, and discharging after staying for a period of time.
The method carries out the step-by-step addition process of the sodium bisulfite and the ethylene oxide, and accurately regulates and controls the process parameters of each step, thereby effectively controlling the hydrolysis rate of the ethylene oxide and the generation of byproducts such as ethylene glycol in the product in the synthesis stage. Avoiding removing impurities by a subsequent complex post-treatment process.
The invention carries out intensive research on the characteristic of the reaction of the sodium bisulfite and the ethylene oxide system through a large number of experiments, the whole process is divided into at least four stages, the pH value in the early stage is lower, and the EO hydrolysis is promoted. Meanwhile, the normal reaction of the sodium bisulfite and EO is not influenced under the condition of large excess of the sodium bisulfite (the EO hydrolysis rate can be controlled at a lower value). In the latter period, as the concentration of sodium bisulfite is gradually reduced, when the feeding amount of the ethylene oxide in the fourth reactor is gradually close to 1 equivalent, but the amount of the EO entering is small, the influence of pH close to neutrality on hydrolysis is small, and the reaction can be promoted to be complete by properly increasing the reaction temperature (the higher the temperature is, the higher the reaction speed of the sodium bisulfite and the EO is promoted).
The whole process is basically carried out under the condition of excessive sodium bisulfite (certain feeding ratio is controlled), the reaction rate of the main reaction of the ethylene oxide is greater than the hydrolysis rate, meanwhile, the temperature and the pH value of different stages are reasonably set, and the temperature is coordinated, so that the hydrolysis of the ethylene oxide can be effectively reduced, the hydrolysis rate is as low as about 0.5 percent (the normal process is generally 1 to 2 percent), the content of the ethylene glycol is lower than 0.1 percent, the content of the polyethylene glycol is extremely low and can be almost ignored, the subsequent treatment and use are greatly facilitated, and the subsequent three-waste treatment amount is reduced. The system is a continuous reaction process and is suitable for industrial production.
The addition reaction is carried out in at least four stages, firstly, sodium bisulfite water solution with certain concentration is mixed with ethylene oxide with certain flow rate at certain flow rate, then the mixture enters from a first reactor, the pH value in the first reactor is regulated and controlled by controlling the flow rate of two raw material solutions, and the retention time of the raw material solutions is about 2-4 h; mixing the first-stage reaction liquid with ethylene oxide at a certain flow rate, then feeding the mixture into a second reactor, controlling the pH value in the second reactor by controlling the flow rate ratio of the initially added sodium bisulfite aqueous solution and the ethylene oxide added at the time, and keeping the reaction liquid for about 1-2 hours, wherein in the way, the reaction liquid respectively enters a third reactor and a fourth reactor, and the keeping time is 1-2 hours respectively; in the fourth reactor, acidic substances are needed to be added to adjust the pH value in the reactor, and the pH value is controlled to be 7.0-8.0. Finally discharging the material, and feeding the material into subsequent crystallization or reaction.
Preferably, the concentration of the sodium bisulfite aqueous solution is 20 to 40wt%; more preferably 30 to 40wt%. Tests show that the preferable concentration of the sodium bisulfite aqueous solution can further promote the conversion of EO and reduce the hydrolysis rate of EO.
In the first stage, the aqueous sodium bisulfite solution is mixed with the ethylene oxide using an in-line static mixer.
In the second to fourth stages, the reaction liquid and the ethylene oxide are mixed by using a pipeline static mixer.
In the first to the fourth stages, in each reactor, the material stirring mode comprises stirring by a stirring paddle or circulating stirring. The reaction is exothermic, and heat exchange operation is required in the reaction process. If stirring by a stirring paddle is adopted, a jacket can be arranged for heat exchange or a built-in coil pipe is arranged for heat exchange operation; if the circulation stirring is adopted, an external heat exchanger can be adopted for heat exchange operation.
Preferably, the acidic substance is selected from sulfur dioxide or sulfurous acid.
From the technical feasibility, the addition reaction can be increased to five stages or even more, but the EO hydrolysis rate and the content of impurities such as ethylene glycol in the product are not greatly reduced, and the addition reaction is preferably carried out in the four stages from the viewpoint of production cost.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a method for producing sodium isethionate by continuous reaction, which optimizes process flow and process parameters on the basis of the existing raw material process, realizes effective control of the hydrolysis rate of ethylene oxide and the generation of byproducts such as ethylene glycol in the product in the synthesis stage, avoids removal of impurities by subsequent complicated post-treatment process, and reduces the subsequent three-waste treatment capacity. The system is a continuous reaction process and is suitable for industrial production.
In the product prepared by the continuous production process, the EO hydrolysis rate is as low as about 0.5%, the ethylene glycol content is lower than 0.1%, and the polyethylene glycol content is extremely low and almost negligible; the yield of the target product of the sodium isethionate is up to 99.5%.
Drawings
FIG. 1 is a schematic diagram of a part of the process for producing sodium isethionate by the continuous reaction used in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
Sodium bisulfite water solution with the mass concentration of 30 percent enters the kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the flow rate of EO is interlocked with the pH value in the kettle 1, and p in the kettle is controlledH is 5.5 to 6.0, EO flow rate control range is 7kg/H to 8.5kg/H, temperature of kettle 1 is controlled to be 30 to 35 ℃, material volume is 195 to 205L, the material is discharged to kettle 2 when the volume is exceeded, EO is simultaneously introduced, EO flow rate is interlocked with pH in kettle 2, pH in kettle is controlled to be 6.0 to 6.5, EO flow rate control range is 0.5kg/H to 2kg/H, temperature of kettle 2 is controlled to be 40 to 45 ℃, material volume is 100 to 105L when the volume is exceeded, the material is discharged to kettle 3 when the volume is exceeded, EO is simultaneously introduced, EO flow rate is interlocked with pH in kettle 3, pH in kettle is controlled to be 6.5 to 7.0, EO flow rate control range is 0.5kg/H to 1kg/H, temperature of kettle 3 is controlled to be 50 to 55 ℃, material volume is 100 to 105L when the volume is exceeded, EO is discharged to kettle 4 and EO is simultaneously introduced, EO flow rate is controlled to be 0.5kg/H to 1kg/H, SO is introduced when the volume is exceeded, SO 2 volume is controlled to be 100 to 105L 2 And interlocking with the pH value in the kettle 4, controlling the pH value in the kettle to be 7.0-8.0, controlling the temperature of the kettle 4 to be 60-65 ℃, controlling the volume of the material to be 105-110L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.08%, the EO hydrolysis rate is 0.5%, and the yield of the sodium isethionate is 99.5%.
Comparative example 1
Sodium bisulfite water solution with the mass concentration of 30 percent enters a reaction kettle at the flow rate of 78.78kg/h, EO is simultaneously introduced, the flow rate of EO is controlled to be 9 kg/h-10 kg/h, the pH value of the solution in the kettle is gradually increased to 6.5-7.0, the reaction temperature is controlled to be 60-65 ℃, after the pH value reaches 6.5-7.0, the flow rate of EO is controlled to be 10kg/h, SO is introduced 2 And interlocked with the pH value in the kettle, controlling the pH value in the kettle to be 7.0-8.0, controlling the volume of the materials in the kettle to be 650-700L, and starting discharging when the volume exceeds the amount.
Through detection, the content of ethylene glycol in the product is 0.28%, the EO hydrolysis rate is 1.76%, and the yield of the sodium isethionate is 98.24%.
Comparative example 2
Sodium bisulfite water solution with the mass concentration of 30 percent enters a reaction kettle 1 at the flow rate of 78.78kg/h, EO is introduced at the same time, the EO flow rate is interlocked with the pH in the kettle 1, the pH in the kettle 1 is controlled to be 6.5 to 7.0 in the first stage, the EO flow rate control range is 9kg/h to 10kg/h, the temperature of the kettle 1 is controlled to be 50 to 55 ℃, the material volume is 500 to 550L, the material is discharged to the kettle 2 when the volume is exceeded, EO is introduced at the same time, the EO flow rate is controlled to be 10kg/h, and the introduction of EO is startedSO 2 And interlocked with the pH value in the kettle, controlling the pH value in the kettle to be 7.0-8.0, controlling the temperature of the kettle 2 to be 60-65 ℃, controlling the volume of the material to be 130-140L, and discharging the material when the volume is exceeded.
The detection shows that the ethylene glycol content in the product is 0.17%, the EO hydrolysis rate is 1.07%, and the yield of the sodium isethionate is 98.93%.
Comparative example 3
Sodium bisulfite water solution with the mass concentration of 30 percent enters a reaction kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 1, the pH in the kettle 1 is controlled to be 5.5-6.0 in the first stage, the EO flow rate control range is 7 kg/h-8.5 kg/h, the temperature of the kettle 1 is controlled to be 30-35 ℃, the material volume is 195-205L, the material is discharged to the kettle 2 when the volume is exceeded, the EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 2, the pH in the kettle is controlled to be 6.0-7.0, the EO flow rate control range is 1 kg/h-2 kg/h, the temperature of the kettle 2 is controlled to be 50-55 ℃, the material volume is 200-210L, the material is discharged to the kettle 3 when the volume is exceeded, the EO flow rate is simultaneously introduced, the EO flow rate is controlled to be 0.5 kg/h-1 kg/h, SO is introduced 2 And interlocking with the pH value in the kettle 3, controlling the pH value in the kettle to be 7.0-8.0, controlling the temperature of the kettle 3 to be 60-65 ℃, controlling the volume of the material to be 105-110L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.1%, the EO hydrolysis rate is 0.63%, and the yield of the sodium isethionate is 99.37%.
Comparative example 4
Sodium bisulfite water solution with the mass concentration of 30 percent enters a kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 1, the pH in the kettle is controlled to be 5.0-5.5, the EO flow rate control range is 7 kg/h-8.5 kg/h, the temperature of the kettle 1 is controlled to be 30-35 ℃, the volume of the material is 195-205L, the material is discharged to the kettle 2 when the volume is exceeded, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 2, the pH in the kettle is controlled to be 5.5-6.0, the EO flow rate control range is 0.5 kg/h-2 kg/h, the temperature of the kettle 2 is controlled to be 40-45 ℃, the volume of the material is 100-105L, the volume is exceeded, the material is discharged to the kettle 3, the EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 3, the pH in the kettle is controlled to be 6.0.0-6.5, the EO flow rate control range is 0.5 kg/h-1 kg/h, the temperature of the kettle 3, the volume of the material is controlled to be 50-55 ℃, the EO flow rate control range is controlled to be 0.5100 to 105L, discharging to the kettle 4 when the volume exceeds the volume, simultaneously introducing EO, controlling the flow rate of the EO to be 0.5kg/h to 1kg/h, and introducing SO 2 And interlocking with the pH value in the kettle 4, controlling the pH value in the kettle to be 6.5-7.0, controlling the temperature of the kettle 4 to be 60-65 ℃, controlling the volume of the material to be 105-110L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.18%, the EO hydrolysis rate is 1.13%, and the yield of the sodium isethionate is 98.87%.
Comparative example 5
Sodium bisulfite water solution with the mass concentration of 30% enters a kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 1, the pH in the kettle is controlled to be 6.0-6.5, the EO flow rate control range is 7 kg/h-8.5 kg/h, the temperature of the kettle 1 is controlled to be 30-35 ℃, the volume of the material is 195-205L, the material is discharged to the kettle 2 when the volume is exceeded, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 2, the pH in the kettle is controlled to be 6.5-7.0, the EO flow rate control range is 0.5 kg/h-2 kg/h, the temperature of the kettle 2 is controlled to be 40-45 ℃, the volume of the material is 100-105L, the volume is exceeded, the volume is discharged to the kettle 3, the EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 3, the pH in the kettle is controlled to be 7.0.0-7.5 kg/h, the EO flow rate control range is 0.5 kg/h-1 kg/h, the temperature of the kettle 3 is controlled to be 50-55 ℃, the volume is simultaneously introduced, the EO flow rate is controlled to be exceeded, the volume is controlled to be 100L, the SO is controlled to be discharged to be 1 h, the volume is controlled to be 1-5, the volume is controlled to be discharged to be 0.5kg/h, the EO flow rate is controlled, the EO flow rate of the kettle is controlled to be 0.5, the EO flow rate controlled 2 And interlocking with the pH value in the kettle 4, controlling the pH value in the kettle to be 7.5-9.0, controlling the temperature of the kettle 4 to be 60-65 ℃, controlling the volume of the material to be 105-110L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.12%, the EO hydrolysis rate is 0.76%, and the yield of the sodium isethionate is 99.24%.
Comparative example 6
Sodium bisulfite water solution with the mass concentration of 30 percent enters a kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the EO flow rate is interlocked with the pH value in the kettle 1, the pH value in the kettle is controlled to be 5.5 to 6.0, the EO flow rate control range is 7kg/h to 8.5kg/h, the temperature of the kettle 1 is controlled to be 40 to 45 ℃, the material volume is 195 to 205L, the material volume exceeds the volume, the material is discharged to the kettle 2, EO is simultaneously introduced, the EO flow rate is interlocked with the pH value in the kettle 2, the pH value in the kettle is controlled to be6.0 to 6.5, EO flow rate control range is 0.5kg/h to 2kg/h, kettle 2 temperature is controlled to be 50 to 55 ℃, material volume is 100 to 105L, the material is discharged to kettle 3 when the volume is exceeded, EO is simultaneously introduced, EO flow rate is interlocked with pH in kettle 3, pH in kettle is controlled to be 6.5 to 7.0, EO flow rate control range is 0.5kg/h to 1kg/h, kettle 3 temperature is controlled to be 60 to 65 ℃, material volume is 100 to 105L, the material is discharged to kettle 4 when the volume is exceeded, EO is simultaneously introduced, EO flow rate is controlled to be 0.5kg/h to 1kg/h, SO is introduced, and 2 and interlocking with the pH value in the kettle 4, controlling the pH value in the kettle to be 7.0-8.0, controlling the temperature of the kettle 4 to be 70-75 ℃, controlling the volume of the material to be 105-110L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.11%, the EO hydrolysis rate is 0.69%, and the yield of the sodium isethionate is 99.31%.
Example 2
Feeding a sodium bisulfite aqueous solution with the mass concentration of 40% into a kettle 1 at the flow rate of 59.09kg/h, simultaneously introducing EO, controlling the EO flow rate to be interlocked with the pH in the kettle 1, controlling the pH in the kettle to be 5.5-6.0, controlling the EO flow rate within the range of 7 kg/h-8.5 kg/h, controlling the temperature of the kettle 1 to be 30-35 ℃, controlling the material volume to be 142-147L, discharging to the kettle 2 when the volume is exceeded, simultaneously introducing EO, controlling the EO flow rate to be interlocked with the pH in the kettle 2, controlling the pH in the kettle to be 6.0-6.5, controlling the EO flow rate within the range of 0.5 kg/h-2 kg/h, controlling the temperature of the kettle 2 to be 40-45 ℃, controlling the material volume to be 70-75L, discharging to the kettle 3 when the volume is exceeded, simultaneously introducing EO, controlling the EO flow rate to be interlocked with the pH in the kettle 3, controlling the pH in the kettle to be 6.5-7.0.5 kg/h, controlling the EO flow rate within the range of 0.5 kg/h-1 kg/h, controlling the temperature of the kettle 3, controlling the EO flow rate to be 50-55 ℃, simultaneously introducing the SO within the volume to be 70-75 h, controlling the volume to be 1kg/h, controlling the material volume to be discharged simultaneously 2 And interlocking with the pH value in the kettle 4, controlling the pH value in the kettle to be 7.0-8.0, controlling the temperature of the kettle 4 to be 60-65 ℃, controlling the volume of the material to be 75-80L, and discharging the material when the volume is over the volume.
Through detection, the content of ethylene glycol in the product is 0.095%, the EO hydrolysis rate is 0.46%, and the yield of the sodium isethionate is 99.54%.
Example 3
118.18kg of a 20% sodium bisulfite aqueous solutionFeeding EO into the kettle 1 at a flow rate of/h, simultaneously feeding EO, interlocking the EO flow rate with the pH value in the kettle 1, controlling the pH value in the kettle to be 5.5-6.0, controlling the EO flow rate to be 7 kg/h-8.5 kg/h, controlling the temperature of the kettle 1 to be 30-35 ℃, controlling the material volume to be 310-315L, discharging the material to the kettle 2 when the volume is exceeded, simultaneously feeding EO, interlocking the EO flow rate with the pH value in the kettle 2, controlling the pH value in the kettle to be 6.0-6.5, controlling the EO flow rate to be 0.5 kg/h-2 kg/h, controlling the temperature of the kettle 2 to be 40-45 ℃, controlling the material volume to be 155-160L, controlling the temperature of the kettle 3 to be 50-55 ℃, simultaneously feeding EO when the EO is fed into the kettle 3, interlocking the EO flow rate with the pH value in the kettle 3, controlling the pH value in the kettle to be 6.5-7.0, controlling the EO flow rate to be 0.5 kg/h-1 kg/h, controlling the temperature of the kettle 3 to be 50-55 ℃, controlling the EO material volume to be 155L, controlling the EO flow rate when the volume is exceeded the volume to be exceeded, discharging the EO flow rate to be 4, simultaneously fed into the EO flow rate of the kettle 1 h 2 And the pH value is interlocked with the pH value in the kettle 4, the pH value in the kettle is 7.0-8.0, the temperature of the kettle 4 is controlled to be 60-65 ℃, the volume of the material is 160-165L, and the material is discharged after the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.06%, the EO hydrolysis rate is 0.54%, and the yield of the sodium isethionate is 99.46%.
Example 4
Sodium bisulfite water solution with the mass concentration of 30% enters a kettle 1 at the flow rate of 78.78kg/h, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 1, the pH in the kettle is controlled to be 5.5-6.0, the EO flow rate control range is 7 kg/h-8.5 kg/h, the temperature of the kettle 1 is controlled to be 25-30 ℃, the volume of the material is 195-205L, the material is discharged to the kettle 2 when the volume is exceeded, EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 2, the pH in the kettle is controlled to be 6.0-6.5, the EO flow rate control range is 0.5 kg/h-2 kg/h, the temperature of the kettle 2 is controlled to be 35-40 ℃, the volume of the material is 100-105L, the volume is exceeded, the volume is discharged to the kettle 3, the EO is simultaneously introduced, the EO flow rate is interlocked with the pH in the kettle 3, the pH in the kettle is controlled to be 6.5-7.0, the EO flow rate control range is 0.5 kg/h-1 kg/h, the temperature of the kettle 3 is controlled to be 45-50 ℃, the volume is simultaneously introduced, the EO flow rate is controlled to be 100L, the SO is controlled to be introduced, the volume is controlled to be 1kg/h, the discharge rate is controlled to be 0.5kg/h, the volume is controlled to be 0.5kg/h, the EO flow rate is controlled to be 0.5-1 kg/h, the volume of the EO flow rate of the kettle is controlled 2 And interlocked with the pH value in the kettle 4, the pH value in the kettle is controlled to be 7.0-8.0, the temperature of the kettle 4 is controlled to be 55-60 ℃, the volume of the material is 105-110L, and the pH value is overAfter the volume is exceeded, discharging is carried out.
Through detection, the content of ethylene glycol in the product is 0.077%, the EO hydrolysis rate is 0.48%, and the yield of the sodium isethionate is 99.52%.
Example 5
Sodium bisulfite water solution with mass concentration of 30 percent enters a reaction kettle 1 at the flow rate of 78.78kg/h, EO is introduced at the same time, the EO flow rate is interlocked with the pH value in the kettle 1, the pH value in the kettle 1 is controlled to be 5.5 to 6.0 in the first stage, the EO flow rate control range is 7kg/h to 8.5kg/h, the temperature of the kettle 1 is controlled to be 30 to 35 ℃, the material volume is 195 to 205L, the material is discharged to the kettle 2 when the volume is exceeded, EO is introduced at the same time, the EO flow rate is interlocked with the pH value in the kettle 2, controlling the pH value in the kettle to be 6.0-6.5, controlling the EO flow rate to be 0.5 kg/h-2 kg/h, controlling the temperature of the kettle 2 to be 40-45 ℃, controlling the material volume to be 100-105L, discharging to the kettle 3 when the EO flow rate exceeds the volume, simultaneously introducing EO, controlling the EO flow rate to be 0.5 kg/h-1 kg/h and interlocking with the pH value in the kettle 3, controlling the pH value in the kettle to be 6.5-7.0, controlling the temperature of the kettle 3 to be 50-55 ℃, controlling the material volume to be 100-105L when the EO flow rate exceeds the volume, discharging to the kettle 4 when the EO flow rate exceeds the volume, simultaneously introducing EO, controlling the EO flow rate to be 0.2 kg/h-0.5 kg/h, introducing SO 2 And interlocked with the pH value in the kettle 4, controlling the pH value in the kettle to be 7.0-7.5, controlling the temperature of the kettle 4 to be 60-65 ℃, controlling the volume of the material to be 60-70L, discharging the material to the kettle 5 when the volume is exceeded, simultaneously introducing EO, controlling the flow rate of the EO to be 0.2 kg/h-0.5 kg/h, introducing SO 2 And interlocking with the pH value in the kettle 5, controlling the pH value in the kettle to be 7.5-8.0, controlling the temperature of the kettle 5 to be 65-70 ℃, controlling the volume of the material to be 60-70L, and discharging the material when the volume is exceeded.
Through detection, the content of ethylene glycol in the product is 0.078%, the EO hydrolysis rate is 0.49%, and the yield of the sodium isethionate is 99.51%.
Claims (3)
1. A method for producing sodium isethionate by continuous reaction takes sodium bisulfite aqueous solution and ethylene oxide as raw materials to carry out addition reaction, and is characterized in that the addition reaction is carried out in at least four stages, and specifically comprises the following steps:
the first stage is as follows: and (2) introducing an aqueous sodium bisulfite solution and ethylene oxide into a first reactor, and controlling the feeding molar ratio of the sodium bisulfite to the ethylene oxide to be 1:0.7 to 0.85, controlling the pH value in the reactor to be 5.5 to 6.0 and the temperature to be 25 to 35 ℃, and discharging after the reactor is kept for a period of time;
the concentration of the sodium bisulfite aqueous solution is 30 to 40wt%;
the retention time of the first stage is 2 to 4 hours;
in the first stage, mixing the sodium bisulfite aqueous solution and the ethylene oxide by adopting a pipeline static mixer;
and a second stage: and (3) introducing the material prepared in the first stage into a second reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the second stage to be 1:0.05 to 0.2, controlling the pH value in the reactor to be 6.0 to 6.5 and the temperature to be 35 to 45 ℃, and discharging after the reactor is kept for a period of time;
the residence time of the second stage is 1 to 2h;
and a third stage: and (3) introducing the material prepared in the second stage into a third reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the third stage to be 1:0.05 to 0.1, controlling the pH value in the reactor to be 6.5 to 7.0 and the temperature to be 45 to 55 ℃, and discharging after the reactor stays for a period of time;
the residence time of the third stage is 1 to 2h;
a fourth stage: and (3) introducing the material prepared in the third stage into a fourth reactor, introducing ethylene oxide, and controlling the feeding molar ratio of the sodium bisulfite in the first stage to the ethylene oxide in the fourth stage to be 1:0.05 to 0.1, adding an acidic substance to adjust the pH value in the reactor to 7.0 to 8.0, keeping the temperature at 55 to 70 ℃, standing for a period of time, and discharging;
the retention time of the fourth stage is 1 to 2h.
2. The method for continuously producing sodium isethionate according to claim 1, wherein in each reactor, the material is agitated by means of stirring paddles or by circulation.
3. The continuous reaction method for producing sodium isethionate according to claim 1, wherein said acidic species is selected from sulfur dioxide or sulfurous acid.
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